US9499451B2 - Soil conditioner compositions containing lignocellulosic biomass fermentation process syrup - Google Patents

Soil conditioner compositions containing lignocellulosic biomass fermentation process syrup Download PDF

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US9499451B2
US9499451B2 US14/510,148 US201414510148A US9499451B2 US 9499451 B2 US9499451 B2 US 9499451B2 US 201414510148 A US201414510148 A US 201414510148A US 9499451 B2 US9499451 B2 US 9499451B2
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syrup
soil
lignocellulosic
agricultural composition
conditioning material
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US20150101378A1 (en
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Steven W Ogle
Stephanie C Vrakas
David William Wood
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Sustainable Technology Corp
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EI Du Pont de Nemours and Co
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    • C05G3/0082—
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00—Other organic fertilisers
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D3/00—Calcareous fertilisers
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D3/00—Calcareous fertilisers
    • C05D3/02—Calcareous fertilisers from limestone, calcium carbonate, calcium hydrate, slaked lime, calcium oxide, waste calcium products
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F5/00—Fertilisers from distillery wastes, molasses, vinasses, sugar plant or similar wastes or residues, e.g. from waste originating from industrial processing of raw material of agricultural origin or derived products thereof
    • C05G3/04—
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
    • C05G3/44—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility for affecting solubility
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/80—Soil conditioners
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J105/00—Adhesives based on polysaccharides or on their derivatives, not provided for in groups C09J101/00 or C09J103/00
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J197/00—Adhesives based on lignin-containing materials
    • C09J197/02—Lignocellulosic material, e.g. wood, straw or bagasse
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K17/00—Soil-conditioning materials or soil-stabilising materials
    • C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
    • C09K17/06—Calcium compounds, e.g. lime
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2405/00—Presence of polysaccharides
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
    • C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel
    • Y02E50/16—

Definitions

  • the invention relates to the field of soil conditioners. More specifically, a lignocellulosic syrup is used as a binder in compositions with agricultural application.
  • the lignocellulosic syrup is a co-product of a lignocellulosic biomass fermentation process
  • Soil conditioners are used to improve the quality of soil for improved plant growth and yield. It is desired that a soil conditioner be applied in a state that is readily dispersed to the soil.
  • active ingredients of soil conditioners are typically in a finely ground or powdery form.
  • the conditioning ingredients are typically combined with a binder to form pellets for ease of handling, transportation, and dispersion to application sites.
  • soil conditioners examples include lime which contains calcium carbonate and other minerals including magnesium, and gypsum which is hydrated calcium sulfate. Lime reduces soil acidity which improves plant growth. Gypsum improves soil drainage and promotes plant growth.
  • lignosulfonate or lignosulfate; sulfonated lignin
  • Lignosulfonate is a by-product of the sulfite method for manufacturing paper from wood pulp. During this process, lignin in wood is separated from cellulose and is sulfonated. The resulting sulfonated lignin by-product is an effective binder for powdery substances.
  • WO201426048 discloses a method for producing a fertilizer wherein pellets of gypsum and a binder, such as lignosulfonate, are made.
  • US20140030369 discloses soil amendment compositions containing lignosulfonate.
  • the invention provides an agricultural composition that is a combination of syrup produced from a fermentation process that initially utilizes lignocellulosic biomass and at least one soil conditioning material.
  • the syrup of the invention is similar in physical properties to the lignosulfonate materials described above but does not require sulfonation and is produced from a process that is environmentally friendly.
  • an agricultural composition comprising:
  • the syrup is a co-product of a process for the production of alcohol from a lignocellulosic biomass.
  • cellulosic syrup has a density of about 1 to about 2 g/cm3 and a viscosity of less than 500 SSU at 100° F. (38° C.).
  • the invention provides a process for the production of an agricultural composition comprising combining the lignocellulosic syrup with at least one soil conditioning material, wherein pellets or granules comprising the syrup and the conditioning material are produced.
  • the invention provides a method for conditioning soil comprising applying an agricultural composition which is described above to the soil.
  • a soil conditioning material is typically prepared as a powdery substance that can disperse and penetrate in the soil to which it is applied.
  • the powdery substance is combined with a binder to form pellets or granules.
  • a syrup produced from a fermentation process that uses lignocellulosic biomass may be used as a binder for powdery soil conditioning materials.
  • the terms “comprises,” “comprising,” “includes,” “including,” “has,” “having,” “contains” or “containing,” or any other variation thereof, are intended to cover a non-exclusive inclusion.
  • a composition, a mixture, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, mixture, process, method, article, or apparatus.
  • “or” refers to an inclusive or and not to an exclusive or. For example, a condition A or B is satisfied by any one of the following: A is true (or present) and B is false (or not present), A is false (or not present) and B is true (or present), and both A and B are true (or present).
  • invention or “present invention” as used herein is a non-limiting term and is not intended to refer to any single embodiment of the particular invention but encompasses all possible embodiments as described in the specification and the claims.
  • the term “about” modifying the quantity of an ingredient or reactant of the invention employed refers to variation in the numerical quantity that can occur, for example, through typical measuring and liquid handling procedures used for making concentrates or use solutions in the real world; through inadvertent error in these procedures; through differences in the manufacture, source, or purity of the ingredients employed to make the compositions or carry out the methods; and the like.
  • the term “about” also encompasses amounts that differ due to different equilibrium conditions for a composition resulting from a particular initial mixture. Whether or not modified by the term “about”, the claims include equivalents to the quantities.
  • the term “about” means within 10% of the reported numerical value, preferably within 5% of the reported numerical value.
  • transferable sugar refers to oligosaccharides and monosaccharides that can be used as a carbon source by a microorganism in a fermentation process.
  • lignocellulosic refers to a composition comprising both lignin and cellulose. Lignocellulosic material may also comprise hemicellulose.
  • cellulosic refers to a composition comprising cellulose and additional components, including hemicellulose.
  • sacharification refers to the production of fermentable sugars from polysaccharides.
  • pretreated biomass means biomass that has been subjected to pretreatment prior to saccharification.
  • the pretreatment may take the form of physical, thermal or chemical means and combinations thereof.
  • butanol refers to isobutanol, 1-butanol, 2-butanol, or combinations thereof.
  • lignocellulosic biomass refers to any lignocellulosic material and includes materials comprising cellulose, hemicellulose, lignin, starch, oligosaccharides and/or monosaccharides. Biomass may also comprise additional components, such as protein and/or lipid. Biomass may be derived from a single source, or biomass can comprise a mixture derived from more than one source; for example, biomass could comprise a mixture of corn cobs and corn stover, or a mixture of grass and leaves.
  • Lignocellulosic biomass includes, but is not limited to, bioenergy crops, agricultural residues, municipal solid waste, industrial solid waste, sludge from paper manufacture, yard waste, wood and forestry waste.
  • biomass examples include, but are not limited to, corn cobs, crop residues such as corn husks, corn stover, grasses (including Miscanthus), wheat straw, barley straw, hay, rice straw, switchgrass, waste paper, sugar cane bagasse, sorghum plant material, soybean plant material, components obtained from milling of grains or from using grains in production processes (such as DDGS: dried distillers grains with solubles), woody material such as trees, branches, roots, wood chips, sawdust, shrubs and bushes, leaves, vegetables, fruits, flowers, empty palm fruit bunch, and energy cane.
  • corn cobs crop residues such as corn husks, corn stover, grasses (including Miscanthus), wheat straw, barley straw, hay, rice straw, switchgrass, waste paper, sugar cane bagasse, sorghum plant material, soybean plant material, components obtained from milling of grains or from using grains in production processes (such as DDGS: dried distillers grains with solubles), woody material such as trees, branches,
  • energy cane refers to sugar cane that is bred for use in energy production. It is selected for a higher percentage of fiber than sugar.
  • lignocellulosic biomass hydrolysate refers to the product resulting from saccharification of lignocellulosic biomass.
  • the biomass may also be pretreated or pre-processed prior to saccharification.
  • lignocellulosic biomass hydrolysate fermentation broth is broth containing product resulting from biocatalyst growth and production in a medium comprising lignocellulosic biomass hydrolysate. This broth includes components of lignocellulosic biomass hydrolysate that are not consumed by the biocatalyst, as well as the biocatalyst itself and product made by the biocatalyst.
  • slurry refers to a mixture of insoluble material and a liquid.
  • a slurry may also contain a high level of dissolved solids. Examples of slurries include a saccharification broth, a fermentation broth, and a stillage.
  • whole stillage refers to the bottoms of a distillation.
  • the whole stillage contains the high boilers and any solids of a distillation feed stream.
  • Whole stillage is a type of depleted broth.
  • liquid stillage refers to a liquid fraction resulting from solid/liquid separation of a whole stillage, fermentation broth, or product depleted fermentation broth.
  • syrup means a concentrated product produced from the removal of water, generally by evaporation, from thin stillage.
  • target product refers to any product that is produced by a microbial production host cell in a fermentation.
  • Target products may be the result of genetically engineered enzymatic pathways in host cells or may be produced by endogenous pathways.
  • Typical target products include but are not limited to acids, alcohols, alkanes, alkenes, aromatics, aldehydes, ketones, biopolymers, proteins, peptides, amino acids, vitamins, antibiotics, and pharmaceuticals.
  • the term “fermentation” refers broadly to the use of a biocatalyst to produce a target product.
  • the biocatalyst grows in a fermentation broth utilizing a carbon source in the broth, and through its metabolism produces a target product.
  • Solids refers to soluble solids and insoluble solids. Solids from a lignocellulosic fermentation process contain residue from the lignocellulosic biomass used to make hydrolysate medium.
  • Volatiles refers herein to components that will largely be vaporized in a process where heat is introduced. Volatile content is measured herein by establishing the loss in weight resulting from heating under rigidly controlled conditions to 950° C. (as in ASTM D-3175). Typical volatiles include, but are not limited to, hydrogen, oxygen, nitrogen, acetic acid, and some carbon and sulfur.
  • Fiberd carbon refers herein to a calculated percentage made by summing the percent of moisture, percent of ash, and percent of volatile matter, and then subtracting that percent from 100.
  • “Ash” is the weight of the residue remaining after burning under controlled conditions according to ASTM D-3174.
  • “Sugars” as referred to in the lignocellulosic syrup composition means a total of monosaccharide and soluble oligosaccharides.
  • Soil conditioning material refers herein to a substance that improves the physical qualities of soil, which may include the ability to provide nutrition for plants.
  • the present agricultural composition contains a lignocellulosic syrup and at least one soil conditioning material.
  • the present lignocellulosic syrup is produced as a co-product from a process that uses lignocellulosic biomass as a source of fermentable sugars which are used as a carbon source for a biocatalyst.
  • the biocatalyst uses the sugars in a fermentation process to produce a target product.
  • the biomass is treated to release sugars such as glucose, xylose, and arabinose from the polysaccharides of the biomass.
  • Lignocellulosic biomass may be treated by any method known by one skilled in the art to produce fermentable sugars in a hydrolysate.
  • the biomass is pretreated using physical, thermal and/or chemical treatments, and saccharified enzymatically.
  • Thermo-chemical pretreatment methods include steam explosion or methods of swelling the biomass to release sugars (see for example WO2010113129; WO2010113130). Chemical saccharification may also be used.
  • Physical treatments for pre-processing the biomass include, but are not limited to, grinding, milling, and cutting.
  • Chemical treatments such as these may be used for particle size reduction prior to further chemical treatment.
  • Chemical treatments include base treatment such as with strong base (ammonia or NaOH), or acid treatment (US8545633; WO2012103220).
  • the biomass is treated with ammonia (U.S. Pat. No. 7,932,063; U.S. Pat. No. 7,781,191; U.S. Pat. No. 7,998,713; U.S. Pat. No. 7,915,017). These treatments release polymeric sugars from the biomass.
  • Particularly useful is a low ammonia pretreatment where biomass is contacted with an aqueous solution comprising ammonia to form a biomass-aqueous ammonia mixture where the ammonia concentration is sufficient to maintain alkaline pH of the biomass-aqueous ammonia mixture but is less than about 12 weight percent relative to dry weight of biomass, and where dry weight of biomass is at least about 15 weight percent solids relative to the weight of the biomass-aqueous ammonia mixture, as disclosed in U.S. Pat. No. 7,932,063, which is herein incorporated by reference.
  • Saccharification which converts polymeric sugars to monomeric sugars, may be either by enzymatic or chemical treatments.
  • the pretreated biomass is contacted with a saccharification enzyme consortium under suitable conditions to produce fermentable sugars.
  • the pretreated biomass Prior to saccharification, the pretreated biomass may be brought to the desired moisture content and treated to alter the pH, composition or temperature such that the enzymes of the saccharification enzyme consortium will be active.
  • the pH may be altered through the addition of acids in solid or liquid form.
  • carbon dioxide (CO 2 ) which may be recovered from fermentation, may be utilized to lower the pH.
  • CO 2 may be collected from a fermenter and fed into the pretreatment product headspace in the flash tank or bubbled through the pretreated biomass if adequate liquid is present while monitoring the pH, until the desired pH is achieved.
  • the temperature is brought to a temperature that is compatible with saccharification enzyme activity, as noted below.
  • suitable conditions may include temperature between about 40° C. and 50° C. and pH between about 4.8 and 5.8.
  • Enzymatic saccharification of cellulosic or lignocellulosic biomass typically makes use of an enzyme composition or blend to break down cellulose and/or hemicellulose and to produce a hydrolysate containing sugars such as, for example, glucose, xylose, and arabinose.
  • Saccharification enzymes are reviewed in Lynd, L. R., et al. (Microbiol. Mol. Biol. Rev., 66:506-577, 2002). At least one enzyme is used, and typically a saccharification enzyme blend is used that includes one or more glycosidases.
  • Glycosidases hydrolyze the ether linkages of di-, oligo-, and polysaccharides and are found in the enzyme classification EC 3.2.1.x (Enzyme Nomenclature 1992, Academic Press, San Diego, Calif. with Supplement 1 (1993), Supplement 2 (1994), Supplement 3 (1995, Supplement 4 (1997) and Supplement 5 [in Eur. J. Biochem., 223:1-5, 1994; Eur. J. Biochem., 232:1-6, 1995; Eur. J. Biochem., 237:1-5, 1996; Eur. J. Biochem., 250:1-6, 1997; and Eur. J. Biochem., 264:610-650 1999, respectively]) of the general group “hydrolases” (EC 3.).
  • Glycosidases useful in saccharification can be categorized by the biomass components they hydrolyze.
  • Glycosidases useful in saccharification may include cellulose-hydrolyzing glycosidases (for example, cellulases, endoglucanases, exoglucanases, cellobiohydrolases, ⁇ -glucosidases), hemicellulose-hydrolyzing glycosidases (for example, xylanases, endoxylanases, exoxylanases, ⁇ -xylosidases, arabino-xylanases, mannases, galactases, pectinases, glucuronidases), and starch-hydrolyzing glycosidases (for example, amylases, ⁇ -amylases, ⁇ -amylases, glucoamylases, ⁇ -glucosidases, isoamylases).
  • peptidases EC 3.4.x.y
  • lipases EC 3.1.1.x and 3.1.4.x
  • ligninases EC 1.11.1.x
  • feruloyl esterases EC 3.1.1.73
  • a “cellulase” from a microorganism may comprise a group of enzymes, one or more or all of which may contribute to the cellulose-degrading activity.
  • Commercial or non-commercial enzyme preparations, such as cellulase may comprise numerous enzymes depending on the purification scheme utilized to obtain the enzyme.
  • Many glycosyl hydrolase enzymes and compositions thereof that are useful for saccharification are disclosed in WO 2011/038019. Additional enzymes for saccharification include, for example, glycosyl hydrolases that hydrolyze the glycosidic bond between two or more carbohydrates, or between a carbohydrate and a noncarbohydrate moiety.
  • Saccharification enzymes may be obtained commercially. Such enzymes include, for example, Spezyme® CP cellulase, Multifect® xylanase, Accelerase® 1500, Accellerase® DUET, and Accellerase® TrioTM (DupontTM/Genencor®, Wilmington, Del.), and Novozyme-188 (Novozymes, 2880 Bagsvaerd, Denmark).
  • saccharification enzymes may be unpurified and provided as a cell extract or a whole cell preparation. The enzymes may be produced using recombinant microorganisms that have been engineered to express one or more saccharifying enzymes.
  • an H3A protein preparation that may be used for saccharification of pretreated cellulosic biomass is an unpurified preparation of enzymes produced by a genetically engineered strain of Trichoderma reesei , which includes a combination of cellulases and hemicellulases and is described in WO 2011/038019, which is incorporated herein by reference.
  • Chemical saccharification treatments may be used and are known to one skilled in the art, such as treatment with mineral acids including HCl and H 2 SO 4 (U.S. Pat. No. 5,580,389; WO2011002660).
  • Sugars such as glucose, xylose and arabinose are released by saccharification of lignocellulosic biomass and these monomeric sugars provide a carbohydrate source for a biocatalyst used in a fermentation process.
  • the sugars are present in a biomass hydrolysate that is used as fermentation medium.
  • the fermentation medium may be composed solely of hydrolysate, or may include components additional to the hydrolysate such as sorbitol or mannitol at a final concentration of about 5 mM as described in U.S. Pat. No. 7,629,156, which is incorporated herein by reference.
  • the biomass hydrolysate typically makes up at least about 50% of the fermentation medium. Typically about 10% of the final volume of fermentation broth is seed inoculum containing the biocatalyst.
  • the medium comprising hydrolysate is fermented in a fermenter, which is any vessel that holds the hydrolysate fermentation medium and at least one biocatalyst, and has valves, vents, and/or ports used in managing the fermentation process.
  • Any biocatalyst that produces a target product utilizing glucose and preferably also xylose, either naturally or through genetic engineering, may be used for fermentation of the fermentable sugars in the biomass hydrolysate made from lignocellulosic biomass.
  • Target products that may be produced by fermentation include, for example, acids, alcohols, alkanes, alkenes, aromatics, aldehydes, ketones, biopolymers, proteins, peptides, amino acids, vitamins, antibiotics, and pharmaceuticals.
  • Alcohols include, but are not limited to methanol, ethanol, propanol, isopropanol, butanol, ethylene glycol, propanediol, butanediol, glycerol, erythritol, xylitol, mannitol, and sorbitol.
  • Acids may include acetic acid, formic acid, lactic acid, propionic acid, 3-hydroxypropionic acid, butyric acid, gluconic acid, itaconic acid, citric acid, succinic acid, 3-hydroxyproprionic acid, fumaric acid, maleic acid, and levulinic acid.
  • Amino acids may include glutamic acid, aspartic acid, methionine, lysine, glycine, arginine, threonine, phenylalanine and tyrosine.
  • Additional target products include methane, ethylene, acetone and industrial enzymes.
  • Biocatalysts may be microorganisms selected from bacteria, filamentous fungi and yeast. Biocatalysts may be wild type microorganisms or recombinant microorganisms, and may include, for example, organisms belonging to the genera of Escherichia, Zymomonas, Saccharomyces, Candida, Pichia, Streptomyces, Bacillus, Lactobacillus , and Clostridiuma .
  • biocatalysts include recombinant Escherichia coli, Zymomonas mobilis, Bacillus stearothermophilus, Saccharomyces cerevisiae, Clostridia thermocellum, Thermoanaerobacterium saccharolyticum , and Pichia stipitis .
  • a biocatalyst may be selected or engineered to have higher tolerance to inhibitors present in biomass hydrolysate such as acetate.
  • the biocatalyst may produce ethanol as a target product, such as production of ethanol by Zymomonas mobilis as described in U.S. Pat. No. 8,247,208, which is incorporated herein by reference.
  • Fermentation is carried out with conditions appropriate for the particular biocatalyst used. Adjustments may be made for conditions such as pH, temperature, oxygen content, and mixing. Conditions for fermentation of yeast and bacterial biocatalysts are well known in the art.
  • saccharification and fermentation may occur at the same time in the same vessel, called simultaneous saccharification and fermentation (SSF).
  • SSF simultaneous saccharification and fermentation
  • partial saccharification may occur prior to a period of concurrent saccharification and fermentation in a process called HSF (hybrid saccharification and fermentation).
  • a smaller culture of the biocatalyst is first grown, which is called a seed culture.
  • the seed culture is added to the fermentation medium as an inoculum typically in the range from about 2% to about 20% of the final volume.
  • fermentation by the biocatalyst produces a fermentation broth containing the target product made by the biocatalyst.
  • the fermentation broth may be a beer containing from about 6% to about 10% ethanol.
  • the fermentation broth contains water, solutes, and solids from the hydrolysate medium and from biocatalyst metabolism of sugars in the hydrolysate medium.
  • the target product is isolated from the fermentation broth producing a depleted broth, which may be called whole stillage.
  • the broth is distilled, typically using a beer column, to generate an ethanol product stream and a whole stillage. Distillation may be using any conditions known to one skilled in the art including at atmospheric or reduced pressure.
  • the distilled ethanol is further passed through a rectification column and molecular sieve to recover an ethanol product.
  • the target product may alternatively be removed in a later step such as from a solid or liquid fraction after separation of fermentation broth.
  • the syrup co-product of a lignocellulosic biomass fermentation process is produced from the fermentation broth or depleted fermentation broth.
  • An example of syrup production is disclosed in US20120102823, which is incorporated herein by reference.
  • the broth or depleted broth, such as whole stillage is separated into solid and liquid streams, where the liquid stream is called thin stillage.
  • Various filtration devices may be used such as a belt filter, belt press, screw press, drum filter, disc filter, Nutsche filter, filter press or filtering centrifuge. Filtration may be aided such as by application of vacuum, pressure, or centrifugal force.
  • a heat treatment may be used as disclosed in commonly owned and co-pending US20120178976, which is incorporated herein by reference.
  • the solids fraction, or filter cake may be burned to supply energy to the production process.
  • the filter cake may be dried prior to burning, such as by air drying, to reduce moisture.
  • a product stream may be removed following liquid/solid filtration of a lignocellulosic biomass hydrolysate fermentation broth.
  • the liquid stream may be extracted or distilled to generate a product stream, such as distillation to produce an ethanol product stream and a remaining liquid.
  • the liquid fraction is further purified by evaporation producing water that may be recycled and a syrup. Prior to evaporation, a portion of the liquid fraction may be recycled for use as back set, which may be added at any point in the process where water is needed, such as in pretreatment, saccharification, or biocatalyst seed production.
  • Evaporation may be in any evaporation system, such as falling film, rising film, forced circulation, plate or mechanical and thermal vapor recompression systems. Evaporation may be continuous or batch and may use a multi-effect evaporator.
  • the evaporated water may be recycled in the overall lignocellulosic biomass hydrolysate fermentation process.
  • the lignocellulosic syrup composition contains from about 40% to about 60% solids or from about 40% to about 70% solids (may have about 40%, 45%, 50%, 55%, 60%, 65%, or 70% solids), from about 10 g/l to 30 g/l of acetamide, at least about 40 g/l of sugars, a density of about 1 to about 2 g/cm 3 , and viscosity less than 500 SSU at 100° F. (38° C.).
  • “SSU” is Saybolt Universal Viscosity in Seconds (Burger V L., Encycl. Ind. Chem. Anal.
  • the lignocellulosic syrup contains at least about 5 g/l of ammonia.
  • a soil conditioning material is combined with the present lignocellulosic syrup to produce the present agricultural composition.
  • a soil conditioning material is a substance that when applied to soil, improves the properties of the soil such that at least one of plant growth and yield are increased. Soil properties that may be improved include, but are not limited to, pH, drainage, providing plant nutrients, soil structure, cation exchange capacity, and water retention. Any soil conditioning material that is mixable may be used in the present invention.
  • the soil conditioning material used is a material that is particulate, and is powdery, dusty, or granular. In one embodiment the soil conditioning material is in the form of a powder.
  • the additional fuel component is lime or gypsum.
  • Lime that is used for soil application is typically crushed or ground limestone which is made of calcium carbonate.
  • Chalk is a form of limestone that is a soft, white, porous sedimentary rock.
  • Dolomitic lime is a type of lime that contains calcium carbonate and magnesium carbonate.
  • Lime is alkaline and is used to neutralize acidity of soil and add calcium, and may add magnesium (if using dolomitic lime).
  • Gypsum is hydrated calcium sulfate. Gypsum removes sodium from soil and replaces it with calcium thereby reducing salinity of soil, and chemically loosens clay soil by competing with salt in the clay thereby improving drainage and plant root growth.
  • the present agricultural composition contains the lignocellulosic syrup described herein and a soil conditioning material, as described above.
  • the lignocellulosic syrup and soil conditioning material are combined in amounts wherein the syrup acts as a binder of the soil conditioning material, which is typically crushed or powdered.
  • the syrup is between about 2% and about 20% by weight of the final combination of syrup and soil conditioning material.
  • the syrup may be about 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20% of the total combined weight.
  • the syrup is between about 2% and 20%, or between about 2% and 10%, of the final composition of syrup and soil conditioning material, and the soil conditioning material is lime, gypsum, or a combination thereof.
  • the lignocellulosic syrup and soil conditioning material are combined in a ratio that is between about 1:50 and about 1:5.
  • the ratio of the lignocellulosic syrup and soil conditioning material may be between about 1:50 and 1:6.7, or between about 1:50 and 1:10.
  • the combination of lignocellulosic syrup and soil conditioning material forms into a conveniently handled solid material.
  • Various shapes may be formed such as pellets, granules, irregular shapes, and the like.
  • the syrup is sprayed over the soil conditioning material in a rotating drum as it rotates.
  • the lignocellulosic syrup and soil conditioning material composition is dried.
  • Alternative processing may include treatments such as heating, compressing, extruding, pelleting, molding, and/or drying.
  • the present agricultural composition is applied to soil by any method known to one skilled in the art.
  • the agricultural composition may be applied by spreading using a conventional fertilizer spreader of any size, such as for lawn care or for agricultural fields.
  • the agricultural composition may be tilled into the soil prior to planting, applied after planting, and/or applied periodically during the growing season.
  • soil testing is performed prior to application to determine the specific type and amount of agricultural composition to be applied to soil.
  • Accellerase® 1500 (A1500) and Multifect® Xylanase are obtained from Danisco U.S. Inc., Genencor, International (Rochester, N.Y.).
  • reesei strain #229 was co-transformed with the ⁇ -xylosidase Fv3A expression cassette (cbh1 promoter, Fv3A gene, cbh1 terminator, and alsR marker), the ⁇ -xylosidase Fv43D expression cassette (egl1 promoter, Fv43D gene, native Fv43D terminator), and the Fv51A ⁇ -arabinofuranosidase expression cassette (egl1 promoter, Fv51A gene, Fv51A native terminator) using electroporation. Transformants were selected on Vogels agar plates containing chlorimuron ethyl.
  • T. reesei integrated expression strain H3A which recombinantly expresses T. reesei ⁇ -glucosidase 1 , T. reesei xyn3, Fv3A, Fv51A, and Fv43D was isolated.”
  • Extra cellular protein produced during fermentation of strain H3A was separated from the cell mass by centrifugation, concentrated by membrane-ultrafiltration through a Millipore 10 kD molecular cut off weight membrane and pH adjusted to 4.8.
  • Total protein was determined using a modified Biuret method as modified by Weichselbaum and Gornall using Bovine Serum Albumin as a calibrator (Weichselbaum, 1960, Amer. J. Clin. Path. 16:40; Gornall et al., 1949 J. Biol. Chem 177:752).
  • This H3A extracellular protein preparation, called herein H3A protein was used as a combination cellulase and hemicellulase preparation effecting complex carbohydrate hydrolysis during SSF.
  • a lignocellulosic biomass hydrolysate fermentation broth may be made using alternative biocatalysts. Exemplary strains are are described below. As an alternative, strain ZW658, deposited as ATCC #PTA-7858, may be used to produce a lignocellulosic biomass hydrolysate fermentation broth for processing.
  • Zymomonas mobilis strain ZW705 was produced from strain ZW801-4 by the methods detailed in U.S. Pat. No. 8,247,208, which is herein incorporated by reference, as briefly restated here. Cultures of Z. mobilis strain ZW801-4 were grown under conditions of stress as follows. ZW801-4 is a recombinant xylose-utilizing strain of Z. mobilis that was described in U.S. Pat. No. 7,741,119, which is herein incorporated by reference. Strain ZW801-4 was derived from strain ZW800, which was derived from strain ZW658, all as described in U.S. Pat. No. 7,741,119.
  • ZW658 was constructed by integrating two operons, PgapxylAB and Pgaptaltkt, containing four xylose-utilizing genes encoding xylose isomerase, xylulokinase, transaldolase and transketolase, into the genome of ZW1 (ATCC #31821) via sequential transposition events, and followed by adaptation on selective media containing xylose.
  • ZW658 was deposited as ATCC #PTA-7858.
  • ZW658 the gene encoding glucose-fructose oxidoreductase was insertionally-inactivated using host-mediated, double-crossover, homologous recombination and spectinomycin resistance as a selectable marker to create ZW800.
  • the spectinomycin resistance marker which was bounded by loxP sites, was removed by site specific recombination using Cre recombinase to create ZW801-4.
  • a continuous culture of ZW801-4 was run in 250 ml stirred, pH and temperature controlled fermentors (Sixfors; Bottmingen, Switzerland).
  • the basal medium for fermentation was 5 g/L yeast extract, 15 mM ammonium phosphate, 1 g/L magnesium sulfate, 10 mM sorbitol, 50 g/L xylose and 50 g/L glucose.
  • Adaptation to growth in the presence of high concentrations of acetate and ammonia was effected by gradually increasing the concentration of ammonium acetate added to the above continuous culture media while maintaining an established growth rate as measured by the specific dilution rate over a period of 97 days. Ammonium acetate was increased to a concentration of 160 mM.
  • Strain AR3 7-31 was produced from strain ZW705 by further adaptation for growth in corn cob hydrolysate medium as disclosed in U.S. Pat. No. 8,476,048, which is incorporated herein by reference.
  • ZW705 was grown in a turbidostat (U.S. Pat. No. 6,686,194; Heurisko USA, Inc. Newark, Del.), which is a continuous flow culture device where the concentration of cells in the culture was kept constant by controlling the flow of medium into the culture, such that the turbidity of the culture was kept within specified narrow limits.
  • Two media were available to the growing culture in the continuous culture device, a resting medium (Medium A) and a challenge medium (Medium B).
  • a culture was grown on resting medium in a growth chamber to a turbidity set point and then was diluted at a dilution rate set to maintain that cell density. Dilution was performed by adding media at a defined volume once every 10 minutes. When the turbidostat entered a media challenge mode, the choice of adding challenge medium or resting medium was made based on the rate of return to the set point after the previous media addition.
  • the steady state concentration of medium in the growth chamber was a mix of Medium A and Medium B, with the proportions of the two media dependent upon the rate of draw from each medium that allowed maintenance of the set cell density at the set dilution rate.
  • a sample of cells representative of the population in the growth chamber was recovered from the outflow of the turbidostat (in a trap chamber) at weekly intervals.
  • the cell sample was grown once in MRM3G6 medium and saved as a glycerol stock at ⁇ 80° C.
  • ZW705 was grown to an arbitrary turbidity set point that dictated that the culture use all of the glucose and approximately half of the xylose present in the incoming media to meet the set point cell density at the set dilution rate.
  • resting medium that was 50% HYAc/YE and 50% MRM3G6.5X4.5NH 4 Ac12.3
  • challenge medium that was HYAc/YE.
  • a strain isolated after 3 weeks was used in another round of turbidostat adaptation using HYAc/YE as the resting medium and HYAc/YE+9 weight % ethanol as the challenge medium.
  • Strain AR3 7-31 was isolated after 2 weeks and was characterized as a strain with improved xylose and glucose utilization, as well as improved ethanol production, in hydrolysate medium. By sequence analysis, AR3 7-31 was found to have a mutation in the Zymomonas mobilis genome ORF encoding a protein having characteristics of a membrane transport protein, and annotated as encoding a fusa
  • Corn stover is milled to 3 ⁇ 8′′ (0.95 cm). Pretreatment is at 140° C. with 14% NH 3 and 65% solids for 60 min. Saccharification is at 47° C., pH 5.3, with 7.8 mg/g glucan+xylan of an enzyme consortium, for 96 hr. Saccharification enzymes are a mix of cellulases and hemicellulases expressed in a Trichoderma reesei strain H3A as described above. The resulting hydrolysate is used in fermentation. 10 mM sorbitol is added to the hydrolysate making the fermentation medium, and the pH is adjusted to 5.8.
  • first frozen strain Zymomonas mobilis AR3 7-31 stock is grown in MRM3G6 (10 g/L BBL yeast extract, 2 g/L KH 2 PO 4 , 1 g/L MgSO 4 *7H 2 O, 60 g/L glucose) at 33° C., without shaking for 8 hr as a revival culture.
  • MRM3G10 medium (same as MRM3G6 but with 100 g/L glucose) is inoculated with revival culture, and incubated at 33° C. with shaking for 14-16 hr. Growth is to an OD 600 between 1.5 and 3.1. The entire culture is used to inoculate a seed fermenter to an initial OD 600 of approximately 0.05.
  • the seed fermentation is carried out in 10 g/L yeast extract, 2 g/L KH 2 PO 4 , 5 g/L MgSO 4 *7H 2 O, 10 mM sorbitol, and 150 g/L glucose. Seed fermentation is performed at 33° C. and pH 5.5. Seed is harvested after first observation of glucose reduction to less than 50 g/L, with glucose measured by using a YSI 2700 SELECTTM Biochemistry Analyzer (YSI Life Sciences; Yellow Springs, Ohio).
  • the seed is added to the hydrolysate medium in the fermenter. Fermentations are carried out at 30° C.-33° C. for 48-72 hr.
  • the fermentation broth is distilled to recover ethanol and the remaining whole stillage is filtered.
  • the liquid fraction is passed through evaporators removing overhead water, and producing a syrup.
  • Raw limestone mined from a quarry in Weeping Water, Nebr. is ground into a fine powder and pneumatically fed into a rotary drum.
  • Syrup produced from a lignocellulosic biomass ethanol production process (see General Methods) is sprayed into the drum filled with the ground limestone as it is rotated.
  • Batches are prepared using syrup as 2 to 10 wt % of the total weight of ground limestone and syrup.
  • the resulting mixture is fed to a dryer and the resulting pellets are allowed to cool and harden.
  • the limestone powder is held together in the resulting solid pellets, with little evidence of powdery material.
  • Raw gypsum mined from a quarry in Fort Dodge, Iowa is ground into a fine powder and pneumatically fed into a rotary drum.
  • Syrup produced from a lignocellulosic biomass ethanol production process (see General Methods) is sprayed into the drum filled with ground gypsum as it is rotated.
  • Batches are prepared using syrup as 2 to 10 wt % of the total weight of ground gypsum and syrup.
  • the resulting mixture is fed to a dryer and the resulting pellets are allowed to cool and harden.
  • the gypsum powder is held together in the resulting solid pellets, with little evidence of powdery material.

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